CN112429763A - Method for large-batch synthesis of cuprous oxide nano-cubic blocks based on continuous kettle type device - Google Patents
Method for large-batch synthesis of cuprous oxide nano-cubic blocks based on continuous kettle type device Download PDFInfo
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- CN112429763A CN112429763A CN202011452830.XA CN202011452830A CN112429763A CN 112429763 A CN112429763 A CN 112429763A CN 202011452830 A CN202011452830 A CN 202011452830A CN 112429763 A CN112429763 A CN 112429763A
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 title abstract description 5
- 238000003786 synthesis reaction Methods 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 22
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 8
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 8
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 8
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000001509 sodium citrate Substances 0.000 claims abstract description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002091 nanocage Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for synthesizing cuprous oxide nano cubic blocks in large batch based on a continuous kettle type device. The method for synthesizing the cuprous oxide nano cube comprises the following steps: 1) preparing a reaction raw material A which is a mixed solution of copper sulfate, sodium citrate and sodium hydroxide, 2) preparing a reaction raw material B which is an ascorbic acid solution, 3) mixing the raw materials through a micro mixer, then feeding the mixed raw materials into a serial continuous reaction kettle for mixing and reaction, collecting reaction products through a collection kettle, and 4) diluting, centrifuging, separating and washing the collected product solution to obtain cuprous oxide nano cubic blocks. The invention realizes the continuous synthesis of cuprous oxide nano cubic blocks, has good stability and high yield, and is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of chemical industry and nano materials, and particularly relates to a method for synthesizing cuprous oxide nano cubic blocks in large batch based on a continuous kettle type device.
Background
Cuprous oxide is a P-type semiconductor material, and many researches on cuprous oxide have been carried out, such as gas sensing, photodegradation, photolysis, and lithium ion batteries. In industrial production, the copper oxide can be used as coating, bactericide, catalyst, flame retardant material, electrode material, information storage material and the like, and the continuous production of the cuprous oxide in industry is of practical and economic significance.
Of the many forms that cuprous oxide has, the nano-cubes represent the most important crystal structure of cuprous oxide, since other concentrated crystal forms (e.g., nanocages, octahedrons, or more complex structures) can be produced by transforming the form of cuprous oxide. However, in recent reports, the synthesis of cubic blocks of cuprous oxide has not been able to achieve good results, such as the generation of some distorted cubic or irregularly shaped by-product particles. In the literature, a large amount of surfactants are used for controlling the morphology, the single reaction time is long, the temperature is often high, the obtained cuprous oxide cubic block is often seriously agglomerated, and the particle size distribution is not good enough. These methods all adopt a batch production method, cannot perform continuous production, and have difficulty in controlling the consistency between batches.
Disclosure of Invention
The invention aims to develop a continuous reaction system and a method for synthesizing a novel nano material, and realizes the efficient, rapid and continuous preparation of the cuprous oxide nano cube.
In order to solve the problems of difficult amplification, low stability, low production efficiency and the like in the existing batch synthesis method, the invention provides the following technical scheme:
the invention provides a method for synthesizing cuprous oxide nano cubic blocks in large batch based on a continuous kettle type device, which comprises the following steps:
1) preparing a reaction raw material A which is a mixed solution of copper sulfate, sodium citrate and sodium hydroxide;
2) preparing a reaction raw material B which is an ascorbic acid solution;
3) mixing the raw material A and the raw material B through a micro mixer to form reaction liquid, allowing the reaction liquid to enter a series-connected continuous reaction kettle for reaction, and collecting a reaction product through a collection kettle;
4) diluting, centrifuging, separating and washing the collected product solution to obtain the cuprous oxide nano cubic material.
Further, the method is characterized in that in the step 1), the content of copper sulfate in the raw material A is 1.5mmol/100mL, the content of sodium citrate is 0.51mmol/100mL, and the content of sodium hydroxide is 25mmol/100 mL; in the step 2), the content of ascorbic acid in the raw material B is 3mmol/100mL, and the feeding volume ratio of the raw material A to the raw material B is 2: 1.
Further, the solvent of the solution of the raw materials A and B is deionized water.
Furthermore, the continuous reaction kettles connected in series are jacketed reaction kettles, the temperature is controlled to be 20-25 ℃ and 30-35 ℃ respectively, and the residence time in the reaction kettles is controlled to be 1-5min and 35-40min respectively.
Further, the time sequence of the step 1) and the step 2) is not sequential, and can also be carried out simultaneously.
Further, the continuous tank apparatus comprises: the device comprises a micro mixer, a continuous reaction kettle and a collection kettle, wherein the continuous reaction kettle and the collection kettle are connected in series, the micro mixer is connected with the continuous reaction kettle, and the continuous reaction kettle is connected with the collection kettle.
Furthermore, the continuous reaction kettles connected in series are jacketed reaction kettles, jackets for heat exchange are arranged outside the inner walls of the continuous reaction kettles, a stirring device is arranged on the continuous reaction kettles, and the collecting kettles are provided with stirrers.
Further, the micro mixer is a caterpillar type micro-channel mixer, a micro-sieve hole dispersing mixer or a vortex mixer; the caterpillar type micro-channel mixer at least comprises a branch intersection channel with the hydraulic diameter of 0.2mm-0.5mm, the micro-sieve pore dispersing mixer at least comprises 1 micro-sieve pore with the diameter of 0.1mm-0.3mm and a corresponding mixing channel, and the eddy type mixer at least comprises an eddy generation area with the diameter of 1mm and a corresponding mixing channel.
The invention solves the problems of difficult amplification, low stability, low production efficiency and the like in the existing batch synthesis method, realizes the continuous synthesis of the up-conversion nano material, and has the following advantages:
1. the new synthesis method can be carried out at near room temperature, and is energy-saving and environment-friendly;
2. the reaction device is operated continuously, the labor cost is low, the production efficiency is high, and the scale-up experiment is easy; a
3. Multi-stage temperature control is favorable for process control, and the safety of the reaction is greatly improved.
Drawings
FIG. 1: the invention relates to a continuous kettle type device for synthesizing cuprous oxide nano cubic blocks.
Detailed Description
The invention will be further elucidated and explained with reference to the embodiments and the drawings.
The invention relates to a continuous kettle type device for synthesizing cuprous oxide nano cubic blocks based on a continuous reaction kettle device, which comprises: 1 micromixer (1), 2 continuous reaction kettles (2, 3) and 1 collection kettle (4), wherein the micromixer (1) is connected with the continuous reaction kettles (2 and 3) which are connected in series, the continuous reaction kettle (3) is connected with the collection kettle (4), and the connection sequence is shown in figure 1.
The process for synthesizing cuprous oxide nano cubic blocks in large batch based on the continuous kettle type device comprises the following steps: mixing a mixed solution (A) containing copper sulfate, sodium citrate and sodium hydroxide with an ascorbic acid solution (B) in a micro mixer (1) to form a reaction solution (C); after flowing out of the micro mixer (1), the reaction liquid (C) flows through the first continuous reaction kettle (2), and the reaction temperature and time are controlled to quickly form precursor reaction liquid (D); the reaction liquid (D) flows out of the first continuous reaction kettle (2), then flows through the second continuous reaction kettle (3), and the reaction temperature and the reaction time are controlled to form reaction liquid (E); and (3) allowing the reaction solution (E) to flow out of the second continuous reaction kettle (3), and collecting the product solution (F) through the collection kettle (4) for subsequent treatment to obtain cuprous oxide nano cubic blocks.
The term "room temperature" as used herein means 15 to 30 ℃.
Examples
A method for synthesizing cuprous oxide nano cubic blocks in large batch based on a continuous kettle type device comprises the following steps:
1) weighing copper sulfate, sodium citrate, sodium hydroxide and ascorbic acid, respectively adding into deionized water at room temperature, and performing ultrasonic treatment until the solution is clear to obtain a mixed solution of copper sulfate, sodium citrate and sodium hydroxide and an ascorbic acid solution.
2) Constructing a continuous reaction kettle device according to the figure 1, conveying the reaction raw materials obtained in the step 1) into a continuous reaction kettle reaction system by using a constant flow pump for reaction, monitoring the temperature of the continuous reaction kettle in real time, and finally collecting the product by using a collection kettle.
3) And sequentially diluting the product solution with deionized water and absolute ethyl alcohol, washing, centrifuging and drying to obtain cuprous oxide nano cubic blocks, and weighing to calculate the yield. The specific experimental conditions and results are as follows:
TABLE 1 tabulation of examples 1-2
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A method for synthesizing cuprous oxide nano cubic blocks in large batch based on a continuous kettle type device is characterized by comprising the following steps:
1) preparing a reaction raw material A which is a mixed solution of copper sulfate, sodium citrate and sodium hydroxide;
2) preparing a reaction raw material B which is an ascorbic acid solution;
3) mixing the raw material A and the raw material B through a micro mixer to form reaction liquid, allowing the reaction liquid to enter a series-connected continuous reaction kettle for reaction, and collecting a reaction product through a collection kettle;
4) diluting, centrifuging, separating and washing the collected product solution to obtain the cuprous oxide nano cubic material.
2. The method as claimed in claim 1), wherein the raw material A in step 1), wherein the content of copper sulfate is 1.5mmol/100mL, the content of sodium citrate is 0.51mmol/100mL, and the content of sodium hydroxide is 25mmol/100 mL; in the step 2), the content of ascorbic acid in the raw material B is 3mmol/100mL, and the feeding volume ratio of the raw material A to the raw material B is 2: 1.
3. The method of claim 1, wherein the solvent of the solution of starting materials a and B is deionized water.
4. The method according to claim 1, wherein the continuous reaction kettles connected in series are jacketed reaction kettles, the temperature is controlled to be 20-25 ℃ and 30-35 ℃ respectively, and the residence time in the reaction kettles is controlled to be 1-5min and 35-40min respectively.
5. The method according to claim 1, wherein the steps 1) and 2) are performed in chronological order, not sequentially, but simultaneously.
6. The method of claim 1, wherein the continuous tank apparatus comprises: the device comprises a micro mixer, a continuous reaction kettle and a collection kettle, wherein the continuous reaction kettle and the collection kettle are connected in series, the micro mixer is connected with the continuous reaction kettle, and the continuous reaction kettle is connected with the collection kettle.
7. The method according to claim 6, wherein the continuous reaction kettles connected in series are jacketed reaction kettles, the jackets for heat exchange are arranged outside the inner walls of the jacketed reaction kettles, the jacketed reaction kettles are provided with stirring devices, and the collecting kettles are provided with stirrers.
8. The method of claim 6, wherein the micromixer is a caterpillar-type microchannel mixer or a micromesh-hole dispersing mixer or a vortex mixer; the caterpillar type micro-channel mixer at least comprises a branch intersection channel with the hydraulic diameter of 0.2mm-0.5mm, the micro-sieve pore dispersing mixer at least comprises 1 micro-sieve pore with the diameter of 0.1mm-0.3mm and a corresponding mixing channel, and the eddy type mixer at least comprises an eddy generation area with the diameter of 1mm and a corresponding mixing channel.
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| CN2020113163695 | 2020-11-20 | ||
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116003989A (en) * | 2022-12-26 | 2023-04-25 | 浙江理工大学 | A kind of antibacterial reinforced waterborne polyurethane composite material and its preparation method and application |
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Application publication date: 20210302 |